CN107434410B - Preparation method of cordierite ceramic powder - Google Patents
Preparation method of cordierite ceramic powder Download PDFInfo
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- CN107434410B CN107434410B CN201710748927.7A CN201710748927A CN107434410B CN 107434410 B CN107434410 B CN 107434410B CN 201710748927 A CN201710748927 A CN 201710748927A CN 107434410 B CN107434410 B CN 107434410B
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- 239000000843 powder Substances 0.000 title claims abstract description 58
- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 27
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000919 ceramic Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims description 13
- 238000005469 granulation Methods 0.000 claims description 11
- 230000003179 granulation Effects 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 238000009694 cold isostatic pressing Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 238000000875 high-speed ball milling Methods 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000395 magnesium oxide Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- -1 magnesium aluminate Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for preparing cordierite ceramic powder, which takes magnesia, alumina and silica powder as raw materials and adopts cordierite (2 MgO.2Al)2O3·5SiO2Or Mg2Al4Si5O18) The chemical components are mixed and reacted to synthesize the high-purity cordierite low-thermal expansion ceramic powder. The preparation process comprises the following steps: firstly, ball milling and mixing high-purity powder; secondly, drying the slurry; thirdly, manually granulating and sieving; fourthly, high-purity cordierite powder is synthesized through high-temperature reaction. The purity of the cordierite powder material obtained by the invention is more than 98%, and the grain diameter of the cordierite powder without refinement treatment is about 20 μm. The cordierite synthesis method adopted by the invention is simple and convenient to operate, can avoid introducing impurities, obtains high-purity powder, is beneficial to the preparation of low-thermal-expansion ceramics in the later period, and is suitable for batch production.
Description
Technical Field
The invention relates to a preparation method of cordierite ceramic powder, belonging to the technical field of ceramic preparation.
Background
Cordierite ceramic is always the preferred material for automobile exhaust purifiers due to excellent thermal shock resistance, higher mechanical strength and chemical corrosion resistance, and has wide application prospect in the field of electronic packaging and the aspect of precise semiconductor component materials. The high-purity and superfine cordierite powder is the key for obtaining the low-thermal expansion ceramic material, and the method for synthesizing the cordierite powder mainly comprises three methods: solid phase reaction, sol-gel, and glass crystallization. In contrast, the solid phase reaction method is the simplest to operate and has the lowest cost; although the sol-gel method can properly reduce the synthesis temperature, the synthesis purity is difficult to control; the glass crystallization method can obtain high-purity cordierite powder under low temperature conditions, but the operation process is complicated, the cost is high, and the industrialization is not facilitated. The solid phase reaction method comprises a natural mineral high-temperature solid phase synthesis method and a high-purity oxide synthesis method, wherein the cordierite powder is synthesized by natural mineral raw materials through solid phase reaction, and the raw materials often contain impurity elements, so that the purity of the synthesized powder is seriously influenced. The high-purity oxide synthesis method has been widely studied because it can synthesize high-purity cordierite powder at a relatively low temperature.
Disclosure of Invention
The invention provides a preparation method of cordierite ceramic powder, aiming at the problems that an impurity phase is easy to appear, the particle size of the powder is too large, the dispersibility of the powder is poor and the like in the existing preparation process of cordierite powder.
The technical scheme for solving the technical problems is as follows:
a method for preparing cordierite ceramic powder comprises the following steps:
1) mixing materials: mixing magnesium oxide, aluminum oxide and silicon oxide powder, wherein the magnesium oxide accounts for 13-14%, the aluminum oxide accounts for 34-35% and the silicon oxide accounts for 51-52% in parts by weight, then placing the mixture into a mixing tank, taking ethanol as a grinding medium, and grinding the mixture in a ball mill under the action of grinding medium balls;
2) and (3) drying: drying the slurry obtained after ball milling;
3) manual granulation and sieving: taking out the dried powder, carrying out cold isostatic pressing forming after vacuum sealing, crushing and sieving to obtain granulation powder with good fluidity;
4) reaction synthesis: placing the granulation powder obtained in the step 3) in an air atmosphere at 1350-1400 ℃ for reaction synthesis;
5) thinning treatment: and then ball-milling the powder obtained in the step 4) to meet the requirement of the required granularity.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the grinding time in the step 1) is 2-6 h.
Further, the grinding medium ball in the step 1) is a zirconia ball.
Further, the drying temperature in the step 2) is 80-100 ℃.
Further, the pressure of the cold isostatic pressing in the step 3) is 60-80 MPa, and the pressure is maintained for 5 s.
Further, the reaction time in the step 4) was 2 hours.
The preparation method has the following beneficial effects:
1) according to the method, the formula offset is increased according to the theoretical chemical formula design, the chemical composition deviates from the theoretical stoichiometric amount, the obtained powder has low crystallization degree, and the powder activity is increased, so that the powder synthesized by the method has the characteristics of high purity and high activity, the high quality stability in batch production can be ensured, and meanwhile, the preparation process of the cordierite low-thermal expansion ceramic has low sintering temperature, and high performance is obtained;
2) the method of the invention has simple operation, can synthesize high-purity cordierite powder at lower temperature, and can obtain low-thermal expansion ceramic powder with high purity, small grain diameter and good dispersibility.
Drawings
FIG. 1 is an XRD spectrum of cordierite powder obtained in examples 1 and 2;
FIG. 2 is an XRD spectrum of a cordierite powder obtained in example 3;
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1:
(1) mixing materials: high-purity MgO and Al with particle sizes of 1 μm, 0.5 μm and 30nm2O3、SiO2Respectively mixing 13.8%, 34.8% and 51.4% by mass, placing in an alumina mixing tank, grinding with ethanol as grinding medium in a planetary ball mill for 4h at high speed under the action of zirconia balls;
(2) and (3) drying: after the mixing is finished, the slurry is placed in a drying oven at 80 ℃ for full drying;
(3) manual granulation and sieving: taking out the dried powder, carrying out cold isostatic pressing under the pressure of 80MPa after vacuum sealing, and then crushing and sieving by a 60-mesh sieve to obtain granulation powder with good fluidity;
(4) reaction synthesis: the granulated powder is placed in an alumina crucible and synthesized by reacting for 2 hours at the high temperature of 1400 ℃ in an oxidizing atmosphere furnace.
(5) Powder thinning treatment: and placing the sintered powder in a ball milling tank for high-speed ball milling to meet the requirement of the required granularity.
The effect of this embodiment: this embodiment can obtain high purity cordierite powder.
Example 2:
(1) mixing materials: high-purity MgO and Al with particle sizes of 1 μm, 0.5 μm and 30nm2O3、SiO2Respectively mixing 13%, 35% and 52% by mass, placing in an alumina mixing tank, taking ethanol as a grinding medium, and grinding for 4h at high speed in a planetary ball mill under the action of zirconia balls;
(2) and (3) drying: after the mixing is finished, the slurry is placed in a drying oven at 80 ℃ for full drying;
(3) manual granulation and sieving: taking out the dried powder, carrying out cold isostatic pressing under the pressure of 80MPa after vacuum sealing, and then crushing and sieving by a 60-mesh sieve to obtain granulation powder with good fluidity;
(4) reaction synthesis: placing the granulated powder in an alumina crucible, and reacting at 1380 ℃ for 2h in an oxidizing atmosphere furnace to synthesize the granulated powder;
(5) powder thinning treatment: and placing the sintered powder in a ball milling tank for high-speed ball milling to meet the requirement of the required granularity.
The effect of this embodiment: this embodiment can obtain high purity cordierite powder.
Example 3:
(1) mixing materials: high-purity MgO and Al with particle sizes of 75 μm, 0.5 μm and 75 μm respectively2O3、SiO2Mixing 14%, 34% and 52% by mass respectively, placing in an alumina mixing tank, taking ethanol as a grinding medium, and grinding for 4h at high speed in a planetary ball mill under the action of zirconia balls;
(2) and (3) drying: after the mixing is finished, the slurry is placed in a drying oven at 100 ℃ for full drying;
(3) manual granulation and sieving: taking out the dried powder, carrying out cold isostatic pressing under the pressure of 60MPa after vacuum sealing, and then crushing and sieving by a 60-mesh sieve to obtain granulation powder with good fluidity;
(4) reaction synthesis: the granulated powder is placed in an alumina crucible and synthesized by reacting for 2 hours at the high temperature of 1350 ℃ in an oxidizing atmosphere furnace.
The effect of this embodiment: this embodiment can obtain a powder having a cordierite phase as a main crystal phase, accompanied by small amounts of magnesium aluminate spinel and silica phases.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (1)
1. A method for preparing cordierite ceramic powder is characterized by comprising the following steps:
(1) mixing materials: high-purity MgO and Al with particle sizes of 1 μm, 0.5 μm and 30nm2O3、SiO2Respectively mixing 13%, 35% and 52% by mass, and placing in an alumina mixing tankTaking ethanol as a grinding medium, and grinding for 4 hours in a planetary ball mill at a high speed under the action of zirconia balls;
(2) and (3) drying: after the mixing is finished, the slurry is placed in a drying oven at 80 ℃ for full drying;
(3) manual granulation and sieving: taking out the dried powder, carrying out cold isostatic pressing under the pressure of 80MPa after vacuum sealing, and then crushing and sieving by a 60-mesh sieve to obtain granulation powder with good fluidity;
(4) reaction synthesis: placing the granulated powder in an alumina crucible, and reacting at 1380 ℃ for 2h in an oxidizing atmosphere furnace to synthesize the granulated powder;
(5) powder thinning treatment: and placing the sintered powder in a ball milling tank for high-speed ball milling to meet the requirement of the required granularity.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110128163B (en) * | 2019-06-26 | 2020-07-24 | 中南大学 | A kind of method for preparing cordierite porous ceramic material using waste catalyst |
| CN112876228A (en) * | 2021-01-26 | 2021-06-01 | 中国兵器工业第五二研究所烟台分所 | High-modulus cordierite-based low-thermal-expansion ceramic and preparation method thereof |
| CN113336479B (en) * | 2021-05-21 | 2023-07-11 | 景德镇陶瓷大学 | A cordierite-based glass-ceramic high-temperature binder and its preparation method and application |
| CN114835511B (en) * | 2022-06-02 | 2023-03-17 | 西安交通大学 | Preparation method of cordierite precursor light-cured paste and porous cordierite ceramics with complex structure |
| CN115321971A (en) * | 2022-09-14 | 2022-11-11 | 浙江天地环保科技股份有限公司 | Method for preparing cordierite ceramic by using fly ash |
| CN116332627A (en) * | 2023-02-14 | 2023-06-27 | 西安航科创星电子科技有限公司 | Low-thermal expansion coefficient high-temperature co-fired ceramic (HTCC) material and preparation method thereof |
| CN117263665B (en) * | 2023-11-21 | 2024-03-12 | 中国科学院上海硅酸盐研究所 | Method for preparing cordierite ceramic by reaction sintering |
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|---|---|---|---|---|
| JPS5112808A (en) * | 1974-07-23 | 1976-01-31 | Asahi Glass Co Ltd | |
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| CN107032774A (en) * | 2017-03-15 | 2017-08-11 | 中国兵器科学研究院宁波分院 | High densification low thermal expansion ceramic preparation method |
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2017
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Inventor after: Zhang Cong Inventor after: Xing Wenfang Inventor after: Lin Guangqing Inventor after: Wang Zhiwei Inventor after: Zhao Bin Inventor after: Zhou Yawei Inventor after: Fang Zhijian Inventor after: Liu Fafu Inventor after: Liang Xiyao Inventor after: Chang Yongwei Inventor after: Jia Shubo Inventor after: Cao Jianwu Inventor after: Li Kang Inventor after: Yang Shuangyan Inventor after: Wang Jinghui Inventor after: Li Guobin Inventor after: Zhang Wu Inventor after: Zhang Tao Inventor after: Guo Jianbin Inventor after: Yan Dongming Inventor after: Gao Xiaoju Inventor after: Li Zhipeng Inventor after: Qiao Guangli Inventor after: Wang Cheng Inventor after: Man Peng Inventor before: Zhang Cong Inventor before: Lin Guangqing Inventor before: Wang Zhiwei Inventor before: Zhao Bin Inventor before: Zhou Yawei Inventor before: Fang Zhijian Inventor before: Liu Fafu Inventor before: Liang Xiyao Inventor before: Chang Yongwei Inventor before: Jia Shubo Inventor before: Li Kang Inventor before: Cao Jianwu Inventor before: Yang Shuangyan Inventor before: Wang Jinghui Inventor before: Li Guobin Inventor before: Zhang Wu Inventor before: Zhang Tao Inventor before: Guo Jianbin Inventor before: Yan Dongming Inventor before: Gao Xiaoju Inventor before: Li Zhipeng Inventor before: Qiao Guangli Inventor before: Wang Cheng Inventor before: Man Peng |
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